CN115612988A - High-magnetic-performance FeGaB magnetoelectric film and preparation method thereof - Google Patents
High-magnetic-performance FeGaB magnetoelectric film and preparation method thereof Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 238000000034 method Methods 0.000 claims description 13
- 238000000151 deposition Methods 0.000 claims description 10
- 238000005137 deposition process Methods 0.000 claims description 8
- 238000004549 pulsed laser deposition Methods 0.000 claims description 7
- 239000002994 raw material Substances 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 9
- 239000010408 film Substances 0.000 description 33
- 239000010409 thin film Substances 0.000 description 7
- 238000012360 testing method Methods 0.000 description 6
- 230000008878 coupling Effects 0.000 description 4
- 238000010168 coupling process Methods 0.000 description 4
- 238000005859 coupling reaction Methods 0.000 description 4
- 238000004544 sputter deposition Methods 0.000 description 4
- 239000007789 gas Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 239000000956 alloy Substances 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 230000010354 integration Effects 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 230000003746 surface roughness Effects 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 230000000875 corresponding effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000012495 reaction gas Substances 0.000 description 1
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- 239000002356 single layer Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/24—Vacuum evaporation
- C23C14/28—Vacuum evaporation by wave energy or particle radiation
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
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- H—ELECTRICITY
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- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F10/00—Thin magnetic films, e.g. of one-domain structure
- H01F10/08—Thin magnetic films, e.g. of one-domain structure characterised by magnetic layers
- H01F10/10—Thin magnetic films, e.g. of one-domain structure characterised by magnetic layers characterised by the composition
- H01F10/12—Thin magnetic films, e.g. of one-domain structure characterised by magnetic layers characterised by the composition being metals or alloys
- H01F10/14—Thin magnetic films, e.g. of one-domain structure characterised by magnetic layers characterised by the composition being metals or alloys containing iron or nickel
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Abstract
The invention discloses a preparation method of a high-magnetic-performance FeGaB magnetoelectric film, which belongs to the technical field of magnetoelectric film materials.
Description
Technical Field
The invention relates to the technical field of magnetoelectric film materials, in particular to a high-magnetic-property FeGaB magnetoelectric film and a preparation method thereof.
Background
The integration and high frequency are the development direction of future magnetic devices. Currently, most magnetic devices are discrete components using bulk materials, which occupy a large space in design and preparation. The magnetoelectric coupling film consists of a magnetostrictive film and a piezoelectric film, and a working mode generated by the magnetoelectric-mechanical-electric dynamic coupling characteristic of the magnetoelectric coupling film can generate very obvious magnetoelectric response at room temperature, thereby providing more design space for the micro-nano integration of a novel magnetic device.
In the magnetostrictive material, the FeGa material has the characteristics of low coercive force, high saturation magnetic induction and large saturation magnetostriction coefficient, and the B element is added into the FeGa material, so that the obtained FeGaB film not only can improve the mechanical property of the FeGa alloy, but also can remarkably optimize the soft magnetic property of the material, and is particularly suitable for resonance application under high-frequency and weak magnetic fields.
In the prior art, magnetron systems of co-sputtering (sputtering of a FeGa target and a B target together) are generally used, such as chinese patent applications CN 111334766A, CN 110777342A, etc. The existing preparation method of the magnetron co-sputtering has the following disadvantages: the film preparation is greatly influenced by environmental factors (voltage instability, ar gas filling flow instability, mutual influence of glow and the like), the atomic ratio of FeGa and B elements in the prepared FeGaB film cannot be stably fixed, the film forming quality is influenced, and the prepared FeGaB film has poor crystallization degree, more large particles and high coercive force. Specifically, the SEM photograph of a typical FeGaB thin film manufactured by the magnetron co-sputtering method is shown in fig. 1, the grain size thereof reaches 150nm, the hysteresis loop thereof is shown in fig. 2, the coercivity thereof reaches 300 Oe, and the surface roughness test result of the thin film by the atomic force microscope is shown in fig. 3, and the roughness thereof reaches 3.751nm.
Therefore, the prior art cannot meet the requirements of preparing the high magnetostriction FeGaB film: the film has excellent magnetic properties of high crystallinity, low coercive force, small roughness and low line width.
Disclosure of Invention
The invention aims to provide a high-magnetic-performance FeGaB magnetoelectric film to solve the problems.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows: a preparation method of a high-magnetic-performance FeGaB magnetoelectric film takes a FeGa target and a B target as raw materials, and is obtained by alternately depositing the FeGa target and the B target by using a Pulsed Laser Deposition (PLD) method.
Compared with the existing magnetron sputtering deposition film, the pulse laser deposition method adopted by the invention does not need to introduce reaction gas during working, and the film can grow under ultrahigh vacuum degree.
As a preferred technical solution, the alternating deposition method is: the FeGa target is firstly subjected to target shooting for 60-75 times and then the B target is subjected to target shooting for 20-26 times in each round.
As a further preferred technical solution, the alternating deposition method is: the FeGa target is firstly targeted 75 times and then the B target is targeted 26 times in each round.
As a preferred technical scheme: the working gas for pulsed laser deposition is KrF.
As a preferred technical scheme: in the pulse laser deposition process, the sample rotation rate is 95-100 degrees/s, and the target rotation rate is 25-35 degrees/s.
As a further preferable technical scheme: in the pulse laser deposition process, the sample rotation rate is 97 degrees/s, and the target rotation rate is 31 degrees/s
As a preferable technical scheme: in the pulse laser deposition process, the laser frequency is 5-10 Hz, and the laser energy is 60-75 mJ.
As a further preferred technical scheme: in the pulse laser deposition process, the laser frequency is 10 Hz, and the laser energy is 75 mJ.
Compared with the prior art, the invention has the advantages that: through the improvement of the preparation method, the prepared film has the advantages of high crystallization degree, low coercive force and small roughness, so that the application requirement of a subsequent novel magnetoelectric device can be met, the magnetostriction capability and the magnetoelectric coupling coefficient of a subsequently manufactured magnetostriction/piezoelectric device are improved, and the application condition is met.
Drawings
FIG. 1 is an SEM photograph of a FeGaB film of the prior art;
FIG. 2 is a hysteresis loop of a FeGaB film of the prior art;
FIG. 3 shows the roughness test results of FeGaB thin films in the prior art;
fig. 4 is an SEM photograph of the FeGaB thin film prepared in example 1 of the present invention;
FIG. 5 is a hysteresis loop of a FeGaB film prepared in example 1 of the present invention;
fig. 6 shows the roughness test results of the FeGaB thin film prepared in example 1 of the present invention.
Detailed Description
The invention will be further explained with reference to the drawings.
Example 1:
a preparation method of a high-magnetic-performance FeGaB magnetoelectric film uses a United states P180 pulse laser deposition system (PLD) to prepare the FeGaB film:
the working gas of the PLD laser in this example is KrF, feGa alloy and B are used as targets (the diameter is 25 mm, the thickness is 5 mm, the purity is more than 99.99 wt%), and the thickness of the substrate Si sheet is 0.3 mm; background vacuum of 1X 10 in the experiment －6 Pa, target distance of 60 mm, sample rotation rate of 97 °/s, target rotation rate of 31 °/s, substrate heating temperature of 200 ℃, laser frequency of 7 Hz, and laser energy of 60 mJ, wherein the FeGaB film is obtained by alternately depositing FeGa targets and B targets, each round of FeGa material is targeted for 60 times, and then the B material is targeted for 20 times, so as to reciprocate;
finally, preparing a FeGaB single-layer film with the thickness of 30nm and the size of 4 inches;
the resulting films were tested as follows:
(1) The results of the test using a scanning electron microscope are shown in fig. 4, and it can be seen from fig. 4 that: the film-forming crystal of the film is compact, the film-forming effect is good, and the grain size is 30nm;
(2) The film structure and the soft magnetic performance are analyzed by using a Vibration Sample Magnetometer (VSM) of an American LakeShore 8600 model, the test result is shown in FIG. 5, and the coercive force of the film is 108 Oe as can be seen from FIG. 5;
(3) The surface roughness test of the thin film was performed using an atomic force microscope, and the result is shown in fig. 6, and it can be seen from fig. 6 that the roughness of the thin film was 0.645nm.
In the present invention, the film property test method and the apparatus used in the prior art are the same as the film property test method of the embodiment.
In other embodiments, the relevant process parameters are adjusted based on the above embodiment 1, and the process parameters and the corresponding properties of the obtained film are shown in table 1:
TABLE 1 Process parameters and Properties of the examples
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (8)
1. A preparation method of a FeGaB magnetoelectric film with high magnetic performance is characterized by comprising the following steps: the method is characterized in that a FeGa target and a B target are used as raw materials, and a pulsed laser deposition method is used for alternately depositing the FeGa target and the B target.
2. The method of claim 1, wherein the alternating deposition method is: the FeGa target is firstly subjected to the target shooting for 60-75 times and then the B target is subjected to the target shooting for 20-26 times in each round.
3. The method of claim 2, wherein the alternating deposition method is: the FeGa target is firstly targeted 75 times and then the B target is targeted 26 times in each round.
4. The method of claim 1, wherein: the working gas for pulsed laser deposition is KrF.
5. The method of claim 1, wherein: in the pulse laser deposition process, the sample rotation rate is 95-100 degrees/s, and the target rotation rate is 25-35 degrees/s.
6. The method of claim 5, wherein: in the pulse laser deposition process, the sample rotation rate is 97 degrees/s, and the target rotation rate is 31 degrees/s.
7. The method of claim 1, wherein: in the pulse laser deposition process, the laser frequency is 5-10 Hz, and the laser energy is 60-75 mJ.
8. The method of claim 1, wherein: in the pulse laser deposition process, the laser frequency is 10 Hz, and the laser energy is 75 mJ.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202211272213.0A CN115612988A (en) | 2022-10-18 | 2022-10-18 | High-magnetic-performance FeGaB magnetoelectric film and preparation method thereof |
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| CN202211272213.0A CN115612988A (en) | 2022-10-18 | 2022-10-18 | High-magnetic-performance FeGaB magnetoelectric film and preparation method thereof |
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Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102683003A (en) * | 2012-05-03 | 2012-09-19 | 中国科学院宁波材料技术与工程研究所 | Method for preparing single-shaft magnetic anisotropy thin film |
| US20120267735A1 (en) * | 2011-04-19 | 2012-10-25 | Jayasimha Atulasimha | Planar Multiferroic/Magnetostrictive Nanostructures as Memory Elements, Two-Stage Logic Gates and Four-State Logic Elements for Information Processing |
| US20160197263A1 (en) * | 2015-01-05 | 2016-07-07 | Inston, Inc. | Systems and Methods for Implementing Efficient Magnetoelectric Junctions |
| CN108389718A (en) * | 2018-02-05 | 2018-08-10 | 电子科技大学 | There is the magnetic bi-layer garnet material and preparation method thereof of the outer direction of easy axis of face inner face simultaneously |
| CN110607503A (en) * | 2019-10-18 | 2019-12-24 | 西南应用磁学研究所 | Soft magnetic composite film for high-frequency magnetic core and preparation method thereof |
| CN110777342A (en) * | 2019-10-22 | 2020-02-11 | 有研工程技术研究院有限公司 | Magnetostrictive film and preparation method thereof |
| CN111334766A (en) * | 2018-12-18 | 2020-06-26 | 有研工程技术研究院有限公司 | Magnetoelectric composite film material and preparation method thereof |
| CN114774858A (en) * | 2022-03-29 | 2022-07-22 | 福建师范大学 | Tunable ferromagnetic resonance composite film and preparation method thereof |
-
2022
- 2022-10-18 CN CN202211272213.0A patent/CN115612988A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20120267735A1 (en) * | 2011-04-19 | 2012-10-25 | Jayasimha Atulasimha | Planar Multiferroic/Magnetostrictive Nanostructures as Memory Elements, Two-Stage Logic Gates and Four-State Logic Elements for Information Processing |
| CN102683003A (en) * | 2012-05-03 | 2012-09-19 | 中国科学院宁波材料技术与工程研究所 | Method for preparing single-shaft magnetic anisotropy thin film |
| US20160197263A1 (en) * | 2015-01-05 | 2016-07-07 | Inston, Inc. | Systems and Methods for Implementing Efficient Magnetoelectric Junctions |
| CN108389718A (en) * | 2018-02-05 | 2018-08-10 | 电子科技大学 | There is the magnetic bi-layer garnet material and preparation method thereof of the outer direction of easy axis of face inner face simultaneously |
| CN111334766A (en) * | 2018-12-18 | 2020-06-26 | 有研工程技术研究院有限公司 | Magnetoelectric composite film material and preparation method thereof |
| CN110607503A (en) * | 2019-10-18 | 2019-12-24 | 西南应用磁学研究所 | Soft magnetic composite film for high-frequency magnetic core and preparation method thereof |
| CN110777342A (en) * | 2019-10-22 | 2020-02-11 | 有研工程技术研究院有限公司 | Magnetostrictive film and preparation method thereof |
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Non-Patent Citations (1)
| Title |
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